#------------------------------------------------------------------------------
#$Date: 2019-11-28 19:56:09 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244455 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/88/7238898.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7238898
loop_
_publ_author_name
'Hashem, Emtithal'
'Swinburne, Adam N.'
'Schulzke, Carola'
'Evans, Rachel C.'
'Platts, James A.'
'Kerridge, Andrew'
'Natrajan, Louise S.'
'Baker, Robert J.'
_publ_section_title
;
 Emission spectroscopy of uranium(iv) compounds: a combined synthetic,
 spectroscopic and computational study
;
_journal_issue                   13
_journal_name_full               'RSC Advances'
_journal_page_first              4350
_journal_paper_doi               10.1039/c3ra22712j
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'Cl4 O2 U, 2(C5 H5 N), 2(C5H6 N)'
_chemical_formula_sum            'C20 H22 Cl4 N4 O2 U'
_chemical_formula_weight         730.25
_chemical_name_common
'bis pyridinium tetrachlorodioxouranate pyridine solvate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.85(3)
_cell_angle_beta                 91.90(3)
_cell_angle_gamma                115.10(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4466(17)
_cell_length_b                   9.1058(18)
_cell_length_c                   9.865(2)
_cell_measurement_reflns_used    2317
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      31.1529
_cell_measurement_theta_min      2.2839
_cell_volume                     621.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      108(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_details
;
scan:
Number of images: 300
Slice: -110.0000 - 40.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 0.0000
Phi: 0.0000
XTD: 44.7245
2theta: -19.7193
scan:
Number of images: 244
Slice: -55.0000 - 67.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 50.0000
Phi: 0.0000
XTD: 44.7245
2theta: -19.7193
scan:
Number of images: 170
Slice: -55.0000 - 30.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 50.0000
Phi: 90.0000
XTD: 44.7245
2theta: -19.7193
scan:
Number of images: 60
Slice: -50.0000 - -20.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 0.0000
Phi: 90.0000
XTD: 44.7245
2theta: -19.7193
;
_diffrn_measurement_device
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6237
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.36
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    6.988
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4796
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             346
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.432
_refine_diff_density_min         -4.142
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0117(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0649P)²+0.8684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                3298
_reflns_number_total             3306
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3ra22712j.txt
_cod_data_source_block           eh1011
_cod_original_cell_volume        621.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7238898
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U1 U 0.5000 1.0000 0.5000 0.02521(12) Uani 1 2 d S
Cl1 Cl 0.6292(2) 1.02487(18) 0.76086(15) 0.0320(3) Uani 1 1 d .
Cl2 Cl 0.6405(2) 0.79001(18) 0.35528(15) 0.0323(3) Uani 1 1 d .
O1 O 0.2997(6) 0.8072(5) 0.4762(5) 0.0303(8) Uani 1 1 d .
N1 N 0.8976(8) 0.7031(7) 0.8833(6) 0.0333(10) Uani 1 1 d .
C1 C 1.0553(9) 0.8420(9) 0.9066(7) 0.0358(12) Uani 1 1 d .
H1 H 1.1428 0.8908 0.9956 0.043 Uiso 1 1 calc R
C2 C 1.0970(9) 0.9181(9) 0.8069(7) 0.0368(13) Uani 1 1 d .
H2 H 1.2124 1.0152 0.8253 0.044 Uiso 1 1 calc R
C3 C 0.9686(10) 0.8512(9) 0.6801(7) 0.0380(14) Uani 1 1 d .
H3 H 0.9934 0.9026 0.6103 0.046 Uiso 1 1 calc R
C4 C 0.8047(10) 0.7093(9) 0.6561(7) 0.0403(14) Uani 1 1 d .
H4 H 0.7134 0.6620 0.5701 0.048 Uiso 1 1 calc R
C5 C 0.7735(9) 0.6356(8) 0.7591(7) 0.0352(12) Uani 1 1 d .
H5 H 0.6613 0.5346 0.7408 0.042 Uiso 1 1 calc R
N2 N 0.1823(8) 0.4499(7) 0.9275(6) 0.0322(10) Uani 1 1 d .
C6 C 0.0673(8) 0.3854(8) 0.7982(7) 0.0331(12) Uani 1 1 d .
H6 H -0.0460 0.2829 0.7727 0.040 Uiso 1 1 calc R
C7 C 0.1119(9) 0.4664(8) 0.7018(7) 0.0336(12) Uani 1 1 d .
H7 H 0.0302 0.4213 0.6103 0.040 Uiso 1 1 calc R
C8 C 0.2778(9) 0.6143(8) 0.7412(7) 0.0332(12) Uani 1 1 d .
H8 H 0.3113 0.6715 0.6759 0.040 Uiso 1 1 calc R
C9 C 0.3948(9) 0.6796(7) 0.8741(7) 0.0348(12) Uani 1 1 d .
H9 H 0.5089 0.7817 0.9018 0.042 Uiso 1 1 calc R
C10 C 0.3432(9) 0.5939(8) 0.9665(6) 0.0327(12) Uani 1 1 d .
H10 H 0.4226 0.6375 1.0588 0.039 Uiso 1 1 calc R
H2N H 0.140(11) 0.379(10) 0.980(9) 0.04(2) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 U1 O1 180.000(1) . 2_676
O1 U1 Cl1 90.21(14) . .
O1 U1 Cl1 89.79(14) 2_676 .
O1 U1 Cl1 89.79(14) . 2_676
O1 U1 Cl1 90.21(14) 2_676 2_676
Cl1 U1 Cl1 180.0 . 2_676
O1 U1 Cl2 90.30(14) . 2_676
O1 U1 Cl2 89.70(14) 2_676 2_676
Cl1 U1 Cl2 88.88(5) . 2_676
Cl1 U1 Cl2 91.12(5) 2_676 2_676
O1 U1 Cl2 89.70(14) . .
O1 U1 Cl2 90.30(14) 2_676 .
Cl1 U1 Cl2 91.12(5) . .
Cl1 U1 Cl2 88.88(5) 2_676 .
Cl2 U1 Cl2 180.0 2_676 .
C1 N1 C5 118.8(5) . .
N1 C1 C2 122.5(6) . .
C3 C2 C1 118.9(6) . .
C4 C3 C2 118.9(6) . .
C3 C4 C5 119.1(6) . .
N1 C5 C4 121.6(6) . .
C6 N2 C10 121.1(5) . .
N2 C6 C7 120.6(6) . .
C6 C7 C8 118.6(6) . .
C9 C8 C7 120.4(5) . .
C8 C9 C10 118.7(6) . .
N2 C10 C9 120.7(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.774(4) .
U1 O1 1.774(4) 2_676
U1 Cl1 2.6523(15) .
U1 Cl1 2.6523(15) 2_676
U1 Cl2 2.6662(16) 2_676
U1 Cl2 2.6662(16) .
N1 C1 1.327(8) .
N1 C5 1.336(9) .
C1 C2 1.377(8) .
C2 C3 1.376(10) .
C3 C4 1.369(10) .
C4 C5 1.389(9) .
N2 C6 1.338(8) .
N2 C10 1.339(8) .
C6 C7 1.379(8) .
C7 C8 1.379(8) .
C8 C9 1.373(9) .
C9 C10 1.376(8) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C5 N1 C1 C2 -0.7(10)
N1 C1 C2 C3 1.9(10)
C1 C2 C3 C4 -1.0(10)
C2 C3 C4 C5 -0.9(10)
C1 N1 C5 C4 -1.3(10)
C3 C4 C5 N1 2.1(10)
C10 N2 C6 C7 -0.1(9)
N2 C6 C7 C8 0.4(9)
C6 C7 C8 C9 -0.5(9)
C7 C8 C9 C10 0.3(10)
C6 N2 C10 C9 -0.1(9)
C8 C9 C10 N2 0.0(9)
